Abstract: A method for the determination of mirex in electrical and electronic products was established by microwave extraction technique and GC/MS. The sample was extracted by microwave with mixed extractant composed of V(n-hexane):V(isopropanol)＝1:1. The extract was purified with silica gel SPE cartridge, and then concentrated. Under the optimum separation and detection condition, mirex was quantified by GC/MS using inner standard method. The recoveries ranged from 82.6% to 106%, with the RSD ranged from 1.6% to 4.3%, and the lower limit of determination could get to the level of 0.5 mg kg^－1. This method is sensitive, accurate and simple to operate.